气体团簇离子束溅射无嵌入法制备用于微化学分析的有机材料截面,Analytical Chemistry

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气体团簇离子束溅射无嵌入法制备用于微化学分析的有机材料截面
Analytical Chemistry ( IF 6.7 ) Pub Date : 2017-04-13 00:00:00 , DOI: 10.1021/acs.analchem.7b00511
Ichiro Mihara _{1,

2} , Rasmus Havelund ₁ , Ian S. Gilmore ₁

Affiliation

我们就地呈现一本小说用于制备有机材料（例如适用于掩埋界面化学成像的聚合物多层膜）横截面的掩模方法。我们在模型掩埋接口系统上演示了该方法，该系统由一块粘附在PET基材上的透明胶带和用于消费者包装的保护膜组成。来自聚焦离子束（FIB）的高剂量镓用于在有机样品的表面上产生损坏的覆盖层。与天然未损坏的有机材料相比，损坏的层的溅射速度要慢得多。因此，在气体团簇离子束（GCIB）深度剖析实验中，损坏的层起着掩模的作用，保护了下面的样品并在掩模的边缘产生了横截面。FIB本身不能直接用于制备横截面，因为有机材料很容易损坏。描述了四个步骤的工作流程，包括最终清洁程序以从横截面上去除重新沉积的材料。对于厚度不超过100μm的样品，该流程将在几个小时内完成。该方法不需要样品嵌入，适合自动分析，这对于常规分析各种样品的工业分析而言可能是重要的好处。

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Embedding-Free Method for Preparation of Cross-Sections of Organic Materials for Micro Chemical Analysis Using Gas Cluster Ion Beam Sputtering

We present a novel in situ mask method for the preparation of cross-sections of organic materials such as polymer multilayer films suitable for chemical imaging of buried interfaces. We demonstrate this method on a model buried interface system consisting of a piece of Scotch tape adhered to a PET substrate and a protective film used in consumer packaging. A high dose of gallium from a focused ion beam (FIB) was used to produce a damaged overlayer on the surface of the organic sample. The damaged layer has a significantly slower sputter rate compared to the native undamaged organic material. Therefore, during gas cluster ion beam (GCIB) depth profiling experiments the damaged layer functions as a mask, protecting the sample beneath and producing a cross-section at the edge of the mask. The FIB itself cannot be used directly to prepare the cross-section since the organic materials are easily damaged. A four step workflow is described including a final cleaning procedure to remove redeposited material from the cross-section. The workflow is completed in a few hours for samples up to 100 μm thickness. The method does not require sample embedding and is suited to automated analysis, which can be important benefits for industrial analysis where a variety of samples are analyzed routinely.

更新日期：2017-04-13

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